CN101613369A - A kind of production technique of oil-free powdery yolk lecithin - Google Patents
A kind of production technique of oil-free powdery yolk lecithin Download PDFInfo
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Abstract
The invention discloses a kind of production technique of oil-free powdery yolk lecithin, in the built-up type stirring tank, utilize the neutral fat in the acetone removal yolk powder earlier, utilize dehydrated alcohol extraction Ovum Gallus domesticus Flavus lecithin wherein again, obtain oil-free powdery yolk lecithin.The invention also discloses the structure of aforesaid combination formula stirring tank.By the oil-free powdery yolk lecithin that the inventive method obtains, acetone insoluble matter content 〉=95%, lecithin content 〉=75%.Technology extraction efficiency height of the present invention, easy and simple to handle, cost is lower, be easy to realization of industrialization.Built-up type stirring tank of the present invention is used in combination paddle stirrer and disc turbine formula agitator, can not make fluid reach the problem of turbulence state very soon to solve single agitator, paddle agitator can make the fluid on top seethe stirring up and down, make the high viscosity fluid reach turbulence state very soon, disc turbine formula agitator can produce the very strong shearing force of convection cell effect, makes the material dispersed effect reach best.
Description
Technical field
The invention belongs to the biochemical engineering technical field, be specifically related to a kind of production technique of oil-free powdery yolk lecithin.
Background technology
Phosphatide is the main composition composition of animal cell membrane system, therefore be to form one of most important basic substance of life, proportion is higher than other system in nerve and internal organ system, and for example: the ratio of phosphatide is high in the seed of brain, liver, yolk, plant etc.Because phosphatide is a kind of biologically active substance, it has unique physical and chemical properties and nutritive value, so phosphatide food, healthcare products, medicine and feedstuff industry worldwide is more and more to be extensive use of.People's edible phospholipid can play and reduce higher blood fat, improves fatty liver symptom, brain tonic and intelligence development and physiological function such as delay senility.
Phosphatide is the general name of the phosphorous lipoid of a class, is made up of mixing such as Yelkin TTS (phosphatidylcholine), kephalin (phosphatidylethanolamine), lipositol (phosphatidylinositols), serine phosphatide (phosphatidylserine), sphingomyelins.Wherein, Yelkin TTS (phosphatidylcholine) is that wherein tool is bioactive a kind of.Yelkin TTS can extract from soybean phospholipid and yolk and yolk powder, be called soybean lecithin and Ovum Gallus domesticus Flavus lecithin, comprehensive and deep processing along with egg product, yolk powder has become the broad range of food raw material, contains 50% the neutral fat of having an appointment, 10% phosphatide and about 40% vitellin(Vt) in the yolk powder of food grade.
At present, extracting Ovum Gallus domesticus Flavus lecithin both at home and abroad and be with fresh yolk liquid or yolk powder is raw material, on the method, is to adopt solvent method, chromatography, membrane sepn and supercritical CO substantially
2Extractions such as method, although the whole bag of tricks is had nothing in common with each other, but it all is identical having a bit, promptly product in the market is paste, desiring to produce the comparatively stable powdery Ovum Gallus domesticus Flavus lecithin of performance still has certain difficulty, and this mainly is cutting performance and degreasing efficient and producing and manufacturing technique and relating to parameters with existing extraction equipment.
CN1884287A discloses a kind of High shear device of using, and is extraction agent with the dehydrated alcohol, and extraction prepares the method for Yelkin TTS.High shear device is for the small-sized extraction kettle in laboratory, have extracting efficient, characteristic of simple, but for the bigger extraction kettle of industrialization, the making of High shear device does not just possess characteristic of simple, with equipment size add ambassador's technology content increase more, thereby the system High shear device is made expense and is also increased greatly.
It is ultrasound-enhanced that CN1974582A discloses a kind of use, with 80%-95% ethanol is the method that extraction agent extracts Yelkin TTS, press the content of document, a kind of really method that improves extraction efficiency of this method, be equally in suitability for industrialized production, with inflammable and explosive organic solvent as aspect the extraction agent, the manufacturing of its ultrasonic device also exists investment more relatively and use the problem of power consumption.
CN10102905A discloses a kind of from egg yolk liquid, the extraction of first edible ethanol to the Yelkin TTS crude product, and then crude product used supercritical CO
2Extraction, deviate to obtain behind the neutral fat 〉=method of 70% Yelkin TTS, though this method is favourable to the biological activity of protection Ovum Gallus domesticus Flavus lecithin, the source of scale operation device raw material need rely on egg product comprehensive process enterprise, in addition, supercritical CO
2Extraction equipment investment also bigger.
It is raw material with fresh yolk liquid that United States Patent (USP) 4.157.404 discloses a kind of, extract the method that obtains egg phospholipids with dme, it obtains moisture earlier and is not more than 20% egg phospholipids, behind the filtration albumen, vacuum concentration obtains moisture and is not more than 1%, the high-quality egg phospholipids of content 50%～85%.
Summary of the invention
Technical problem to be solved by this invention provides a kind of production technique of oil-free powdery yolk lecithin, to produce the powdery Ovum Gallus domesticus Flavus lecithin of stable performance.
The technical problem that the present invention also will solve provides employed a kind of specific equipment in the above-mentioned technology, i.e. built-up type stirring tank, this stirring tank have higher shear performance and strong mass transfer ability.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of production technique of oil-free powdery yolk lecithin comprises the steps:
(1) remove neutral fat in the yolk powder:
(1a) in the built-up type stirring tank, with yolk powder and acetone by weight (kg) volume (L) mixed 5～60 minutes than 1: 1～15;
(1b) the mixture solid-liquid separation that step (1a) is obtained, (way of recycling is a batch distillation in liquid portion (being acetone) recycling, the tower still is a grease), yolk powder repeating step (1a) and (1b) the operation 1～8 time of solid part in replacement step (1a);
(1c) solid part that obtains of step (1b) obtained not having oily yolk powder in 1～4 hour through vacuum-drying;
(2) extraction Ovum Gallus domesticus Flavus lecithin:
(2a) in the built-up type stirring tank, the nothing oil yolk powder that step (1c) is obtained and dehydrated alcohol (kg) volume (L) by weight compare 1: 1～10, mix 5～60 minutes;
(2b) the mixture solid-liquid separation that step (2a) is obtained, liquid portion is retained standby, nothing oil yolk powder repeating step (2a) in the solid part replacement step (2a) and operation (2b) 1～2 time;
(2c) liquid portion that obtains of combining step (2b), vacuum concentration to lecithin content is 30%～90%, ethanol is recycled;
(2d) concentrated solution that step (2c) is obtained, vacuum-drying 1～4 hour;
(2e) the dry thing cooling back of step (2d) is pulverized, promptly get oil-free powdery yolk lecithin.
In the step (1a), the weight of yolk powder and acetone (kg) volume (L) is than preferred 1: 3～6.
In the step (2a), weight (kg) volume (L) that does not have oily yolk powder and dehydrated alcohol is than preferred 1: 5～8.
Step (1a) or (2a) in, preferred 10～20 minutes of the time that mixes.
Step (1b) or (2b) in, solid-liquid separating method is centrifugal, solid-liquid separation method is centrifugal or suction filtration or filter press.
Step (1c) or (2d) in, the vacuum-drying temperature is 10 ℃～80 ℃.
In the step (2c), the vacuum concentration temperature is 10 ℃～80 ℃.
Raw material yolk powder of the present invention is commercially available common fresh yolk powder, requires the manufacturer must not add any additive in yolk powder, as: talcum powder, trimeric cyanamide, starch or starch conversion product etc.
Since the different different solubility of phosphatide in ethanol, the solubleness maximum of Yelkin TTS in ethanol, and kephalin takes second place.So the inventive method uses ethanol as solvent, enrichment obtains Ovum Gallus domesticus Flavus lecithin from yolk powder.Contain 50% the neutral fat of having an appointment in the yolk powder of food grade, 10% phosphatide and about 40% vitellin(Vt), use acetone, remove earlier that to contain 50% the neutral fat of having an appointment in the yolk powder very necessary, so just improved Yelkin TTS and wrapped up the state that is difficult for stripping by a large amount of neutral fats, ensured the content of the acetone insoluble matter of Ovum Gallus domesticus Flavus lecithin, significantly reduce the alcoholic acid usage quantity simultaneously, therefore, yolk powder is directly related with the de-oiling effect in the dispersion state of acetone, also with the de-oiling yolk powder in the ethanol of Yelkin TTS extraction yield and efficient directly related, so, use dynamical equipment, the reinforcing mass transfer ability, improve the dispersion state of yolk powder in solvent, to improve the Yelkin TTS yield, cutting down the consumption of energy and cost, and shorten the extraction time, is characteristics of the present invention.
Employed built-up type stirring tank comprises the reactor that is equipped with agitator and baffle plate in the inventive method, and the stir shaft of described agitator is vertically arranged with two-layer agitator, and wherein, the upper strata is a paddle stirrer, and lower floor is a disc turbine formula agitator.
Wherein, the blade of described paddle stirrer is a hinging type.
Wherein, the blade of described disc turbine formula agitator is an arrow leaf formula.
Wherein, described baffle number is 4, radially is provided with along reactor, is evenly distributed on the reactor inwall, is in the stirring region substantially.
The optimal technical scheme of aforesaid combination formula stirring tank is: stirring tank is the stainless steel stirring tank of 500～5000 liters of volumes, and the stirring tank aspect ratio is 1: 1.2～0.8, and the ratio of stirring tank internal diameter and stirrer diameter is 2～6: 1; The space internal diameter that baffle plate surrounds in reactor is 0.8～0.9: 1 with reactor internal diameter ratio, single height of baffle plate is 0.6～1: 1 with the ratio of kettle height, the thickness of single baffle plate is 2～5mm, and the spacing between described baffle plate and the inner wall of kettle is 0～0.008: 1 with reactor internal diameter ratio.The diameter of stir shaft is 40～80mm; The wheel hub of paddle stirrer is provided with 2 blades, blade vertical with stir shaft and with the angle of horizontal plane be 30 °～90 °, vane thickness is 1～5mm, width of blade is 60～120mm; The wheel hub of disc turbine formula agitator is provided with 6 groups of blades, and every group is that 30 °～90 ° blade is formed (being arrow leaf formula) by 2 angles, and vane thickness is 1～5mm, and width of blade is 60～120mm.
A more preferred scheme of aforesaid combination formula stirring tank is: stirring tank is the stainless steel stirring tank of 1500～2500 liters of volumes, and the stirring tank aspect ratio is 1: 1, and the ratio of stirring tank internal diameter and stirrer diameter is 3～5: 1; The space internal diameter that baffle plate surrounds in reactor is 0.85～0.86: 1 with reactor internal diameter ratio, single height of baffle plate is 0.8～0.9: 1 with the ratio of kettle height, the thickness of single baffle plate is 3～4mm, and the spacing between described baffle plate and the inner wall of kettle is 0～0.005: 1 with reactor internal diameter ratio; The diameter of stir shaft is 50～70mm; The wheel hub of paddle stirrer is provided with 2 blades, blade vertical with stir shaft and with the angle of horizontal plane be 45 °～60 °, vane thickness is 3～4mm, width of blade is 80～100mm; The wheel hub of disc turbine formula agitator is provided with 6 groups of blades, and every group is that 45 °～60 ° blade is formed by 2 angles, and vane thickness is 3～4mm, and width of blade is 80～100mm.
Alleged in this specification sheets " internal diameter ", " directly " etc. are all diameter.
When using single disc turbine formula agitator, stirring system is when stirring the high viscosity fluidic, because the incipient ratio of viscosities of fluid is bigger, after agitator often occurring and starting for some time, just near the direction that stirs along with agitator of the fluid the agitator is done circumference and is flowed, what stirring tank was interior is in relative static conditions from agitator fluid far away, particularly liquid level; When using single paddle agitator, though can adopt hinged joint slurry formula impeller, axial flow that also can convection cell has certain effect, because this agitator speed is generally not high, and makes the fluidic convection circulation relatively poor.
For the suspension operation of solid matter at liquid material; the purpose of agitator is that solid is evenly distributed; thereby chemical processes such as dissolving are finished in the requirement by technology; under the turning effort of agitator; make solid particulate obtain certain movement velocity; be suspended in the liquid phase to overcome its extreme settling velocity; the principal element of decision solid particulate suspension degree in liquid material is the turbulent extent of liquid; it is flow rate of fluid; for the liquid in the still; same when using single disc turbine formula agitator; it is to be difficult to accomplish higher stirring rank that the circumference mobile is only arranged; also be difficult to obtain bigger shearing force, thereby be difficult to obtain higher efficient and yield.After adopting built-up type agitator of the present invention, owing to given full play to the advantage of paddle agitator and disc turbine formula agitator, reach the fluid that makes away from agitator and seethed stirring up and down, make high stickiness fluid reach turbulence state very soon, and the very strong shearing force of convection cell effect, make the material dispersed effect reach best, manifest characteristics aspect higher saving energy consumption, easy operation, efficient.
Beneficial effect: by the oil-free powdery yolk lecithin that the inventive method obtains, acetone insoluble matter content 〉=95%, lecithin content 〉=75%, its concrete technical parameter sees Table 1.The powdery Ovum Gallus domesticus Flavus lecithin of producing more helps post-production than the paste Ovum Gallus domesticus Flavus lecithin on the existing market.Technology extraction efficiency height of the present invention, easy and simple to handle, cost is lower, easy
The performance of common paste product relatively on table 1 products and marketing of the present invention
In realization.Built-up type stirring tank of the present invention is used in combination paddle stirrer and disc turbine formula agitator, can not make fluid reach the problem of turbulence state very soon to solve single agitator, paddle agitator can make the fluid on top seethe stirring up and down, make the high viscosity fluid reach turbulence state very soon, disc turbine formula agitator can produce the very strong shearing force of convection cell effect, makes the material dispersed effect reach best.
Description of drawings
Fig. 1 is a combination stirring-type reactor synoptic diagram of the present invention.
Fig. 2 is the baffle plate vertical view.
Fig. 3 is the front view of disc turbine formula agitator among the present invention.
Fig. 4 is the vertical view of disc turbine formula agitator among the present invention.
Fig. 5 for the A of the blade-section of disc turbine formula agitator among the present invention to view.
Embodiment:
According to following embodiment, the present invention may be better understood.Yet, those skilled in the art will readily understand that the described concrete material proportion of embodiment, processing condition and result thereof only are used to illustrate the present invention, and should also can not limit the present invention described in detail in claims.
Fig. 1 is preferred example of the present invention.
The built-up type stirring tank is the stainless steel stirring tank of 2000 liters of volumes, comprise the reactor 1 that is equipped with agitator and baffle plate 2, agitator is rotatable under the effect of variable-frequency motor 3, the stir shaft of described agitator is vertically arranged with two-layer agitator, wherein, the upper strata is a paddle stirrer 4, and lower floor is a disc turbine formula agitator 5.
The stirring tank aspect ratio is 1: 1, and the ratio of stirring tank internal diameter and stirrer diameter is 3.5.The diameter of stir shaft is 65mm.The blade of paddle stirrer 4 is a hinging type, is arranged with 2 blades on the wheel hub, blade vertical with stir shaft and with the angle of horizontal plane be 45 °, vane thickness is 4mm, width of blade is 100mm; The blade of disc turbine formula agitator 5 is an arrow leaf formula, wheel hub is provided with 6 groups of blades (Fig. 3～4), every group is that 60 ° blade is formed (Fig. 5) by 2 angles, vane thickness is 4mm, width of blade is 100mm, the blade sense of rotation is opposite with the leaf angle bearing of trend, is to flow to the arrow tail by arrow to guarantee flow direction.Because blade is slightly curved, its section is parabolic, thereby two strands of oblique cycling streams are up and down axially arranged, and is low in energy consumption, and has higher shearing force.
Baffle number is 4, radially is provided with along reactor, and evenly vertical distribution is in the stirring region substantially at the reactor inwall, and promptly baffle plate is divided reactor equally and is the quartern, as shown in Figure 2.The space internal diameter that baffle plate surrounds in reactor is 0.85: 1 with reactor internal diameter ratio, single height of baffle plate is 0.85: 1 with the ratio of kettle height, the thickness of single baffle plate is 4mm, and the spacing between described baffle plate and the inner wall of kettle is 0.003: 1 with reactor internal diameter ratio.
Following examples are all used above-mentioned 2000 liters stainless steel stirring tank.
The employed raw material yolk powder of following examples is available from Dalian Hanwei Foods Co., Ltd..
Embodiment 1:
(1) remove neutral fat in the yolk powder:
(1a) in the built-up type stirring tank, inject 1200L acetone, turn on agitator adds the 300Kg yolk powder simultaneously, mixes 20 minutes;
(1b) mixture that step (1a) is obtained is centrifugal, and liquid portion (being acetone) is recycled, and solid part is put into the built-up type stirring tank again, injects 1200L acetone, re-extract lock out operation 2 times;
(1c) solid part (having passed through extracting operation 3 times) that obtains of step (1b) place vacuum dryer, vacuum tightness be-0.06～-0.095MP, drying temperature is 50 ℃, dry 4 hours, altogether 150.7 kilograms of no oily yolk powders;
(2) extraction Ovum Gallus domesticus Flavus lecithin:
(2a) in the built-up type stirring tank, inject 1000L ethanol, turn on agitator adds the nothing oil yolk powder that step (1c) obtains simultaneously, mixes 10 minutes;
(2b) mixture that step (2a) is obtained is centrifugal, and liquid portion is retained standby, and solid part is put into the built-up type stirring tank again, re-extract lock out operation 1 time;
(2c) two portions liquid of obtaining of combining step (2b), 50～60 ℃ of thickening temperatures, vacuum concentration to lecithin content is 62.5%, 63.2 kilograms of concentrated solutions, ethanol is recycled;
(2d) concentrated solution that step (2c) is obtained is by 2 kilograms of drip pans of packing into of every dish, and vacuum tightness is-0.06～-0.095MPa, 50 ℃, dried 1 hour;
(2e) the dry thing cooling back of step (2d) is pulverized, promptly get 38.9 kilograms of oil-free powdery yolk lecithins.
Embodiment 2:
(1) remove neutral fat in the yolk powder:
(1a) in the built-up type stirring tank, inject 1000L acetone, turn on agitator adds the 300Kg yolk powder simultaneously, mixes 10 minutes;
(1b) mixture that step (1a) is obtained is centrifugal, and liquid portion (being acetone) is recycled, and solid part is put into the built-up type stirring tank again, injects 1000L acetone, re-extract lock out operation 1 time;
(1c) solid part (having passed through extracting operation 2 times) that obtains of step (1b) place vacuum dryer, vacuum tightness be-0.06～-0.095MP, 60 ℃, dry 3 hours, altogether 172.3 kilograms of no oily yolk powders;
(2) extraction Ovum Gallus domesticus Flavus lecithin:
(2a) in the built-up type stirring tank, inject 1000L ethanol, turn on agitator adds the nothing oil yolk powder that step (1c) obtains simultaneously, mixes 20 minutes;
(2b) mixture that step (2a) is obtained is centrifugal, and liquid portion is retained standby, and solid part is put into the built-up type stirring tank again, re-extract lock out operation 2 times;
(2c) three partially liqs that obtain of combining step (2b), thickening temperature is 60 ℃～70 ℃, vacuum concentration to lecithin content is 71.5%, 59.5 kilograms of concentrated solutions, ethanol is recycled;
(2d) concentrated solution that step (2c) is obtained is by 2 kilograms of drip pans of packing into of every dish, and vacuum tightness is-0.06～-0.095MPa, drying temperature is 70 ℃, dries 3 hours;
(2e) the dry thing cooling back of step (2d) is pulverized, promptly get 37.5 kilograms of oil-free powdery yolk lecithins.
Claims (10)
1, a kind of production technique of oil-free powdery yolk lecithin is characterized in that this method comprises the steps:
(1) remove neutral fat in the yolk powder:
(1a) in the built-up type stirring tank, with yolk powder and acetone by weight (kg) volume (L) mixed 5～60 minutes than 1: 1～15;
(1b) the mixture solid-liquid separation that step (1a) is obtained, liquid portion be through recycling, yolk powder repeating step (1a) and (1b) the operation 1～8 time of solid part in replacement step (1a);
(1c) solid part that obtains of step (1b) obtained not having oily yolk powder in 1～4 hour through vacuum-drying;
(2) extraction Ovum Gallus domesticus Flavus lecithin:
(2a) in the built-up type stirring tank, nothing oil yolk powder that step (1c) is obtained and dehydrated alcohol (kg) volume (L) by weight mixed 5～60 minutes than 1: 1～10;
(2b) the mixture solid-liquid separation that step (2a) is obtained, liquid portion is standby through retaining, oily yolk powder repeating step (2a) of the nothing of solid part in replacement step (2a) and operation (2b) 1～2 time;
(2c) liquid portion that obtains of combining step (2b) is 30%～90% through vacuum concentration to lecithin content, and ethanol is recycled;
(2d) concentrated solution that step (2c) is obtained, vacuum-drying 1～4 hour;
(2e) the dry thing cooling back of step (2d) is pulverized, promptly get oil-free powdery yolk lecithin.
2, the production technique of oil-free powdery yolk lecithin according to claim 1, it is characterized in that step (1a) or (2a) in, the time of mixing is 5～60 minutes.
3, the production technique of oil-free powdery yolk lecithin according to claim 1, it is characterized in that step (1b) or (2b) in, solid-liquid separating method is centrifugal or suction filtration or filter press.
4, the production technique of oil-free powdery yolk lecithin according to claim 1, it is characterized in that step (1c) or (2d) in, the vacuum-drying temperature is 10 ℃～80 ℃.
5, the production technique of oil-free powdery yolk lecithin according to claim 1 is characterized in that in the step (2c) that the vacuum concentration temperature is 10 ℃～80 ℃.
6, a kind of built-up type stirring tank comprises the reactor that is equipped with agitator and baffle plate, it is characterized in that the stir shaft of described agitator is vertically arranged with two-layer agitator, and wherein, the upper strata is a paddle stirrer, and lower floor is a disc turbine formula agitator.
7, built-up type stirring tank according to claim 6, the blade that it is characterized in that described paddle stirrer is a hinging type; The blade of described disc turbine formula agitator is an arrow leaf formula.
8, built-up type stirring tank according to claim 6 is characterized in that quantity is 4, radially is provided with along reactor, is evenly distributed on the reactor inwall, is in the stirring region substantially.
9, according to any described built-up type stirring tank in the claim 6～8, it is characterized in that, stirring tank is the stainless steel stirring tank of 500～5000 liters of volumes, and the stirring tank aspect ratio is 1: 1.2～0.8, and the ratio of stirring tank internal diameter and stirrer diameter is 2～6: 1; The space internal diameter that baffle plate surrounds in reactor is 0.8～0.9: 1 with reactor internal diameter ratio, single height of baffle plate is 0.6～1: 1 with the ratio of kettle height, the thickness of single baffle plate is 2～5mm, and the spacing between described baffle plate and the inner wall of kettle is 0～0.008: 1 with reactor internal diameter ratio.
10, built-up type stirring tank according to claim 9, the diameter that it is characterized in that stir shaft is 40～80mm; The wheel hub of paddle stirrer is provided with 2 blades, blade vertical with stir shaft and with the angle of horizontal plane be 30 °～90 °, vane thickness is 1～5mm, width of blade is 60～120mm; The wheel hub of disc turbine formula agitator is provided with 6 groups of blades, and every group is that 30 °～90 ° blade is formed by 2 angles, and vane thickness is 1～5mm, and width of blade is 60～120mm.
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